CN103309152A - Resist pattern formation method, pattern formation method, solar cell and positive resist composition - Google Patents
Resist pattern formation method, pattern formation method, solar cell and positive resist composition Download PDFInfo
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- CN103309152A CN103309152A CN2013100765901A CN201310076590A CN103309152A CN 103309152 A CN103309152 A CN 103309152A CN 2013100765901 A CN2013100765901 A CN 2013100765901A CN 201310076590 A CN201310076590 A CN 201310076590A CN 103309152 A CN103309152 A CN 103309152A
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Abstract
The present invention provides a resist pattern formation method. The method includes: a step of applying a positive resist composition on a support containing a substrate of a solar cell so as to form a resist film, wherein the positive resist includes a novolac resin (A) and a photosensitizer (B), and the transmissivity of light with a wavelength of 365 nm in the film formed by the positive resist with a thickness of 3 [mu]m is more than 10%, wherein the photosensitizer (B) includes ester compounds containing a phenol (B1) of tri(hydroxyphenyl) methane skeleton and a sulfonyl compound (B2) with quinone diazide groups; a step of selectively irradiating the resist film for exposure; and a step of developing the resist film after exposure with an alkaline solution, and removing the exposed part.
Description
Technical field
Used eurymeric corrosion-resistant composition in the manufacturing of formation method, the pattern forming method in supporting mass that has used this resist pattern, the solar cell with this figure and the solar cell of used resist pattern when the supporting mass that the present invention relates to comprise the used for solar batteries substrate carries out etching.
Background technology
The technology of solar cell substrate being carried out partly etch processes in the manufacturing process of solar cell is disclosed in the patent documentation 1.In addition, disclose in the patent documentation 2 and 3 when solar cell substrate carried out etch processes as the employed eurymeric corrosion-resistant composition of mask agent.
The prior art document
Patent documentation
Patent documentation 1: No. 3100901 communique of Jap.P.
Patent documentation 2: TOHKEMY 2010-176012 communique
Patent documentation 3: the international pamphlet that discloses No. 2010/013642
Above-mentioned eurymeric corrosion-resistant composition contains emulsion, has by this emulsion only to make exposure section soluble characteristic in developer solution.In addition, emulsion exerts an influence to the photopermeability of the etchant resist that is made of the eurymeric corrosion-resistant composition, and when the content of emulsion increased, the photopermeability of etchant resist can diminish.
On the other hand, solar cell substrate, be formed at the coating object of the eurymeric corrosion-resistant compositions such as electrode on the solar cell substrate, diffusion layer, antireflection film, that is, in general the supporting mass of resist pattern has concavo-convex on the surface.The etchant resist that is coated with the eurymeric corrosion-resistant composition and forms is compared with the protuberance on supporting mass surface, becomes large at recess place thickness.Like this, with regard to the part on the recess that is laminated in supporting mass of etchant resist, light is difficult to arrive the interface of etchant resist and supporting mass.Therefore, etchant resist is difficult to carry out photoresponse at the recess of supporting mass, thereby can't obtain enough dissolution velocities.Thus, etchant resist creates a difference aspect the dissolution velocity because of the difference of thickness.Consequently, the trend that everywhere easily reduces in deciduous at the recess of supporting mass of etchant resist.
Summary of the invention
The present invention finishes in view of such problem, and its purpose is, the technology of deciduous of the etchant resist at the recess place that can realize improving supporting mass is provided.
The formation method that a kind of mode of the present invention is a kind of resist pattern.The formation method of this resist pattern is characterised in that, comprising: the eurymeric corrosion-resistant composition is coated on the supporting mass that comprises solar cell substrate and forms the operation of etchant resist; Etchant resist is optionally shone light and the operation of exposing; And the etchant resist after will exposing with alkaline solution develops and operation that exposed portion is removed; Wherein, described eurymeric corrosion-resistant composition contains novolac resin (A) and emulsion (B) and the optical transmission rate of the wavelength 365nm of the etchant resist of the thickness 3 μ m that formed by described eurymeric corrosion-resistant composition is more than 10%, and described emulsion (B) contains the phenols (B1) with three (hydroxyphenyl) methane skeleton and the ester compounds that contains the sulfonyl compound (B2) of quinone diazido.
According to aforesaid way, can improve the deciduous of etchant resist at the recess place of supporting mass.
In the formation method of the resist pattern of aforesaid way, phenols (B1) can be by following formula (1) or following formula (2) expression.
[in formula (1), (2), R
B1～R
B5Be the alkyl of hydrogen atom, carbon number 1～10 or the alkyl of ring-type independently of one another; R
B6Be hydrogen atom or methyl; P is 1 or 2.]
In addition, containing the sulfonyl compound (B2) of quinone diazido can be by the expression of following formula (3) or following formula (4).
[in formula (3) and the formula (4), R is hydrogen atom, chlorine atom or methyl.]
Another kind of mode of the present invention is a kind of pattern forming method.This pattern forming method comprises: the resist pattern that the formation method of the resist pattern by any above-mentioned mode is formed is as mask, and the supporting mass that will comprise partly solar cell substrate carries out etched operation.
Another kind of mode of the present invention is a kind of solar cell.This solar cell comprises the figure that forms by above-mentioned pattern forming method.
Another kind of mode of the present invention is a kind of eurymeric corrosion-resistant composition.This eurymeric corrosion-resistant composition is characterised in that; the optical transmission rate of the wavelength 365nm of the etchant resist of the thickness 3 μ m that contain novolac resin (A) and emulsion (B), formed by described eurymeric corrosion-resistant composition is more than 10%, be used for the manufacturing of solar cell; wherein, described emulsion (B) contains the phenols (B1) with three hydroxyphenyl methane skeletons and the ester compounds that contains the sulfonyl compound (B2) of quinone diazido.
Description of drawings
Fig. 1 among Fig. 1 (A)～Fig. 1 (D) is the process profile for the manufacturing process of explanation solar cell.
Fig. 2 among Fig. 2 (A)～Fig. 2 (D) is the process profile for the manufacturing process of explanation solar cell.
Fig. 3 among Fig. 3 (A)～Fig. 3 (C) is the process profile for the manufacturing process of explanation solar cell.
Embodiment
Below will be based on preferred embodiment the present invention will be described.Embodiment does not limit invention and is illustration, and all features described in the embodiment or its are combined the content of the essence that not exclusively is invention.
The eurymeric corrosion-resistant composition of present embodiment is the eurymeric corrosion-resistant composition that when the manufacturing of solar cell, for example preferably uses when the supporting mass that comprises solar cell substrate is carried out etch processes partly.The eurymeric corrosion-resistant composition of present embodiment contains: novolac resin (A) and the emulsion (B) that contains phenols (B1) with three hydroxyphenyl methane skeletons and the ester compounds of the sulfonic acid (B2) that contains the quinone diazido, and the optical transmission rate of the wavelength 365nm of the etchant resist of the thickness 3 μ m that formed by described eurymeric corrosion-resistant composition is more than 10%, more preferably more than 11%.Thus, can improve the deciduous of etchant resist at the recess place of supporting mass.The upper limit of the optical transmission rate of the wavelength 365nm of the etchant resist of thickness 3 μ m is not particularly limited, yet is preferably below 30%.
Below, each composition of the eurymeric corrosion-resistant composition that consists of present embodiment is elaborated.
＜novolac resin (A) 〉
As novolac resin (A), can enumerate following illustrative phenols and following illustrative aldehydes are reacted under the acidic catalysts such as hydrochloric acid, sulfuric acid, formic acid, oxalic acid, p-toluenesulfonic acid and novolac resin etc.
As phenols, for example can enumerate phenol; The cresols classes such as metacresol, paracresol, orthoresol; 2,3-xylenols, 2,5-xylenols, 3, the dimethylbenzene phenols such as 5-xylenols, DMP; M-ethylphenol, paraethyl phenol, o-ethyl phenol, 2,3,5-pseudocuminol, 2,3,5-triethyl phenol, 4-TBP, 3-tert-butyl phenol, 2-TBP, 2-tert-butyl-4-methyl-Phenol, the 2-tert-butyl group-alkyl benzene phenols such as 5-methylphenol; P methoxy phenol, meta-methoxy phenol, to thanatol, m-oxethyl phenol, to alkoxy benzene phenols such as propoxyl group phenol, m-phenoxy phenol; Adjacent isopropenyl phenol, to isopropenyl phenol, 2-methyl-4-isopropenyl phenol, the 2-ethyl-isopropenylbenzene phenols such as 4-isopropenyl phenol; The aryl phenol classes such as phenylphenol; 4, the polyhydroxy benzenes phenols such as 4 '-dihydroxybiphenyl, bisphenol-A, resorcinol, p-dihydroxy-benzene, 1,2,3,-thrihydroxy-benzene etc.They both may be used singly or in combination of two or more.In these phenols, particularly preferably metacresol, paracresol.
As aldehydes, such as enumerating formaldehyde, paraformaldehyde, trioxymethylene (trioxane), acetaldehyde, propionic aldehyde, butyraldehyde, trimethyl-acetaldehyde, acryl aldehyde, crotonaldehyde, hexamethylene aldehyde (cyclohexane aldehyde), furfural, furylacrolein, benzaldehyde, terephthalaldehyde, phenyl acetaldehyde, α-hydrocinnamicaldehyde, beta-phenyl propionic aldehyde, salicylaldhyde, m-hydroxybenzaldehyde, parahydroxyben-zaldehyde, o-tolualdehyde, a tolyl aldehyde, p-tolyl aldehyde, o-chlorobenzaldehyde, m chlorobenzaldehyde, 4-chloro-benzaldehyde, cinnamic acid etc.They both may be used singly or in combination of two or more.In these aldehydes, consider preferred formaldehyde from the easness that obtains.
Novolac resin (A) both can be made of a kind of novolac resin, also can be made of the novolac resin more than 2 kinds.In the situation that novolac resin (A) is made of the novolac resin more than 2 kinds, the Mw of each novolac resin is not particularly limited, yet preferably whole as novolac resin (A) and so that weight-average molecular weight (Mw) reaches 1000～100000 mode is prepared.It should be noted that, novolac resin (A) preferably contains 20～70 quality % in the eurymeric corrosion-resistant composition.
As common characteristic in novolac resin discussed above (A), can enumerate the acid resistance excellence.
＜emulsion (B) 〉
Emulsion (B) contains the phenols (B1) with three hydroxyphenyl methane skeletons and the ester compounds that contains the sulfonic acid (B2) of quinone diazido.More particularly, emulsion (B) contains the phenols (B1) with three hydroxyphenyl methane skeletons and the ester compounds that contains the sulfonyl compound (B2) of naphthoquinones diazido by following formula (1) or (2) expression.
[in formula (1), (2), R
B1～R
B5Be the alkyl of hydrogen atom, carbon number 1～10 or the alkyl of ring-type independently of one another; R
B6Be hydrogen atom or methyl; P is 1 or 2.]
More specifically example by the phenols (B1) of formula (1) expression is three (4-hydroxyphenyl) methane, two (4-hydroxyls-3, the 5-3,5-dimethylphenyl)-4-hydroxyphenyl methane, two (4-hydroxyls-2, the 5-3,5-dimethylphenyl)-4-hydroxyphenyl methane, two (4-hydroxyls-3, the 5-3,5-dimethylphenyl)-2-hydroxyphenyl methane, two (4-hydroxyls-2, the 5-3,5-dimethylphenyl)-2-hydroxyphenyl methane, two (4-hydroxyls-2, the 5-3,5-dimethylphenyl)-3,4-dihydroxyphenyl methane, and two (4-hydroxyls-3, the 5-3,5-dimethylphenyl)-3, three (hydroxyphenyl) methane class or its methyl substitutes such as 4-dihydroxyphenyl methane, perhaps two (3-cyclohexyl-4-hydroxyphenyl)-3-hydroxyphenyl methane, two (3-cyclohexyl-4-hydroxyphenyl)-2-hydroxyphenyl methane, two (3-cyclohexyl-4-hydroxyphenyl)-4-hydroxyphenyl methane, two (5-cyclohexyl-4-hydroxy-2-methyl phenyl)-2-hydroxyphenyl methane, two (5-cyclohexyl-4-hydroxy-2-methyl phenyl)-3-hydroxyphenyl methane, two (5-cyclohexyl-4-hydroxy-2-methyl phenyl)-4-hydroxyphenyl methane, two (3-cyclohexyl-2-hydroxyphenyl)-3-hydroxyphenyl methane, two (5-cyclohexyl-4-hydroxy-3-methyl phenyl)-4-hydroxyphenyl methane, two (5-cyclohexyl-4-hydroxy-3-methyl phenyl)-3-hydroxyphenyl methane, two (5-cyclohexyl-4-hydroxy-3-methyl phenyl)-2-hydroxyphenyl methane, two (3-cyclohexyl-2-hydroxyphenyl)-4-hydroxyphenyl methane, two (3-cyclohexyl-2-hydroxyphenyl)-2-hydroxyphenyl methane, two (5-cyclohexyl-2-hydroxy-4-methyl phenyl)-2-hydroxyphenyl methane, and two (cyclohexyl hydroxyphenyl) (hydroxyphenyl) methane classes such as two (5-cyclohexyl-2-hydroxy-4-methyl phenyl)-4-hydroxyphenyl methane or its methyl substitute.
More specifically example by the phenols (B1) of formula (2) expression is 4,4 '-1-[4-(2-(4-hydroxyphenyl)-2-propyl group) phenyl] and ethylidene } bis-phenol or 3,3 '-dimethyl-1-[4-(2-(3-methyl-4-hydroxyphenyl)-2-propyl group) phenyl] and ethylidene } bis-phenol.
As the sulfonyl compound that contains the naphthoquinones diazido (B2); for example can enumerate by 1 of following formula (3) expression; 2-naphthoquinones-2-diazido-5-sulfonyl compound or by 1 of following formula (4) expression, 2-naphthoquinones-2-diazido-4-sulfonyl compound.
[in formula (3) and the formula (4), R is hydrogen atom, chlorine atom or methyl.]
Phenols (B1) with three hydroxyphenyl methane skeletons can heat to carry out by an amount of raw material is dissolved in the water with the esterification that contains the sulfonic acid (B2) of quinone diazido.
In addition, the content of emulsion (B) is preferably the scope of 1～30 quality % for the gross mass of eurymeric corrosion-resistant composition.Thus, can realize more reliably the raising of deciduous of etchant resist at the recess place of supporting mass.
＜other composition 〉
The eurymeric corrosion-resistant composition can contain solvent (C), sensitizer (D), surfactant (E), other adjuvant etc. as other composition.
(solvent (C))
The eurymeric corrosion-resistant composition preferably is dissolved in novolac resin (A) and emulsion (B) in the suitable solvent (C), and is used with the form of solution.As the example of this kind solvent (C), can enumerate the ethylene glycol alkyl ethers such as glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol ether and ethylene glycol monobutyl ether; The diglycol dialkyl ethers such as diethylene glycol dimethyl ether, diethyl carbitol, diglycol dipropyl ether and diethylene glycol dibutyl ether; The ethylene glycol alkyl ether acetate esters such as methylcellosolve acetate, ethyl cellosolve acetate and diethylene glycol monoethyl ether acetic acid esters; The propylene glycol alkyl ether acetic acid ester classes such as propylene glycol methyl ether acetate, propylene glycol monoethyl ether acetate and propylene glycol monopropyl ether acetic acid esters; The ketones such as acetone, MEK, cyclohexanone and methyl amylketone; Toluene and dimethylbenzene etc. are aromatic hydrocarbon based; The ring type ethers such as diox; And the ester classes such as 2 hydroxy propanoic acid methyl esters, 2 hydroxy propanoic acid ethyl ester, 2-hydroxy-2-methyl ethyl propionate, ethoxy ethyl acetate, oxo ethyl acetate, 2-hydroxy-3-methyl methyl butyrate, 3-methoxyl butylacetic acid ester, 3-methyl-3-methoxyl butylacetic acid ester, ethyl formate, ethyl acetate, butyl acetate, methyl acetoacetate and ethyl acetoacetate etc.These solvents both can be used alone, but also also mix together more than 2 kinds.
It should be noted that, obtain for example thickness more than the 3 μ m in order to use spin-coating method, and preferably use solid component concentration in the eurymeric corrosion-resistant composition to reach the solvent (C) of the following amount of the above 65 quality % of 20 quality %.
(sensitizer (D))
The eurymeric corrosion-resistant composition can contain sensitizer (D).Operable sensitizer (D) is not particularly limited in the present embodiment, can at random select in the normally used sensitizer from the eurymeric corrosion-resistant composition.As such sensitizer (D), can enumerate in skeleton structure, have pseudocuminol or carbazole and not with the oxybenzene compound of the sulfonyl compound generation esterification that contains the naphthoquinones diazido.In addition, can enumerate the phenol body (ProductName TrisP-PA-MF (Honshu chemical company system)) etc. of 4-tomatotone (4CPA).
In addition, as sensitizer (D), can use the oxybenzene compound by following formula (D-1) expression.
[in the following formula (D-1), R
41～R
48Represent independently of one another hydrogen atom, halogen atom, the carbon number alkyl below 6, the carbon number alkoxy below 6 or naphthenic base more than 1 more than 1; R
49R
51Represent independently of one another hydrogen atom or the carbon number alkyl below 6 more than 1; Q represents hydrogen atom, the carbon number alkyl below 6 and R more than 1
49The several rings below 6 or by the residue of following formula (D-2) expression more than 3 of bonding and the carbochain that forms; W, s represent the integer below 3 more than 1; U represents the integer below 3 more than 0; V represents the integer below 3 more than 0.]
[in the following formula (D-2), R
52And R
53Represent independently of one another hydrogen atom, halogen atom, the carbon number alkyl below 6, the carbon number alkoxy below 6 or naphthenic base more than 1 more than 1; T represents the integer below 3 more than 1.]
As the oxybenzene compound by following formula (D-1) expression, for example can enumerate two (4-hydroxyls-2,3, the 5-trimethylphenyl)-2-hydroxyphenyl methane, 1,4-is two, and [1-(3,5-dimethyl-4-hydroxyphenyl) isopropyl] benzene, 2,4-two (3,5-dimethyl-4-hydroxyphenyl methyl)-the 6-methylphenol, two (4-hydroxyls-3, the 5-3,5-dimethylphenyl)-2-hydroxyphenyl methane, two (4-hydroxyls-2, the 5-3,5-dimethylphenyl)-2-hydroxyphenyl methane, two (4-hydroxyls-3, the 5-3,5-dimethylphenyl)-3,4-dihydroxyphenyl methane, 1-[1-(4-hydroxyphenyl) isopropyl]-4-[1, two (4-hydroxyphenyl) ethyls of 1-] benzene, 1-[1-(3-methyl-4-hydroxyphenyl) isopropyl]-4-[1, two (3-methyl-4-hydroxyphenyl) ethyls of 1-] benzene, 2,6-is two, and [1-(2, the 4-dihydroxyphenyl) isopropyl]-the 4-methylphenol, 4, two [1-(4-hydroxyphenyl) isopropyl] resorcinols of 6-, 4,6-two (3,5-dimethoxy-4 '-hydroxyphenyl methyl) 1,2,3,-thrihydroxy-benzene, 4,6-two (3,5-dimethyl-4-hydroxyphenyl methyl) 1,2,3,-thrihydroxy-benzene, 2, two (the 3-methyl-4 of 6-, 6-dihydroxyphenyl methyl)-the 4-methylphenol, 2,6-two (2,3,4-three hydroxyphenyl methyl)-the 4-methylphenol, and two (4-hydroxyphenyl) cyclohexanes of 1,1-etc.In addition, in addition, can also use 6-hydroxyl-4a-(2, the 4-dihydroxyphenyl)-and 9-1 '-spirocyclohexyl-1,2,3,4,4a, 9a-six hydrogen xanthenes and 6-hydroxy-5-methyl base-4a-(2,4-dihydroxy-3-aminomethyl phenyl)-9-1 '-spirocyclohexyl-1,2,3,4,4a, 9a-six hydrogen xanthenes etc.These sensitizers both can use separately, also can mix use two or more, yet 1-[1-(4-hydroxyphenyl) isopropyl wherein]-4-[1, two (4-hydroxyphenyl) ethyls of 1-] benzene and two (4-hydroxyls-2,3, the 5-trimethylphenyl)-and the perpendicularity aspect that is combined in high-sensitivity and space diagram of 2-hydroxyphenyl methane is excellent, considers and preferred from this point.
In addition, as sensitizer (D), can use the oxybenzene compound by following formula (D-3) expression.
[in the following formula (D-3), R
61～R
63Represent independently of one another low alkyl group, naphthenic base or lower alkoxy; Q and r represent more than 1 below 3 independently of one another, preferred integer below 2 more than 1; 1, o and p represent the integer below 3 more than 0 independently of one another.]
Here, R
61～R
63Represented low alkyl group and lower alkoxy both can be that the straight chain shape also can be chain, were preferably carbon number more than 1 below 5, carbon number more than 1 below 3 more preferably.In addition, R
61～R
63Represented naphthenic base is preferably carbon number more than 5 below 7.
As the compound by following formula (D-3) expression, more particularly, can enumerate the compound by following formula (D-4)～(D-8) expression.
In addition, as sensitizer (D), can use the oxybenzene compound by following formula (D-9) expression.
[in the following formula (D-9), R
71～R
79Represent independently of one another hydrogen atom, alkyl, halogen atom or hydroxyl, R
71～R
79In at least one be hydroxyl.R
80～R
85Represent independently of one another hydrogen atom, alkyl, alkenyl, naphthenic base or aryl.]
Here, R
71～R
74In at least one and R
75～R
79In at least one be preferably hydroxyl.In addition, R
71～R
79Represented alkyl both can be the straight chain shape, also can be chain, was preferably carbon number more than 1 below 5, carbon number more than 1 below 3 more preferably.And then, R
80～R
85Represented alkyl both can be the straight chain shape, also can be chain, was preferably carbon number more than 1 below 10; As R
80～R
85Represented alkenyl is preferably carbon number more than 1 below 4.
As the oxybenzene compound by following formula (D-9) expression, more particularly, can enumerate the compound by following formula (D-10) expression.
[in the following formula (D-10), R
86And R
87Represent independently of one another alkyl, f and g represent more than 1 below 3, are preferably the integer below 2 more than 1, and j and z represent the integer below 3 more than 0.]
Here, R
86And R
87Represented alkyl both can be the straight chain shape, also can be chain, was preferably carbon number more than 1 below 5, carbon number more than 1 below 3 more preferably.
As the oxybenzene compound by following formula (D-9) expression, more particularly, can enumerate by following formula (D-11) and reach (D-12) compound of expression.
The content of sensitizer (D) is preferably 1～10 quality % for the gross mass of eurymeric corrosion-resistant composition, more preferably 2～5 quality %.
(surfactant (E))
The described eurymeric corrosion-resistant composition of embodiment can contain the surfactant (E) of fluorine system, silicon system or acrylic acid series.
As the surfactant (E) of fluorine system, can enumerate KL-600 (common prosperity society chemistry system) etc.As the surfactant (E) of silicon system, can enumerate with the polyester modification dimethyl silicone polymer as the BYK-310 (Byk-Chemie system) of major component, with the poly-methyl alkyl siloxane of aralkyl modification as the BYK-323 (Byk-Chemie system) of major component, with the dimethyl silicone polymer of polyether-modified hydroxyl as the BYK-SILCLEAN3720 (Byk-Chemie system) of major component etc.In addition, as the surfactant (E) of acrylic acid series, can enumerate BYK-354 (Byk-Chemie system).In the middle of them, the surfactant (E) that preferred silicon is, the more preferably surfactant (E) of dimethyl silicone polymer system.The content of surfactant (E) is preferably 0.001 quality %～1.0 quality % for the gross mass of eurymeric corrosion-resistant composition, more preferably 0.01 quality %～0.1 quality %.
(other adjuvant)
The described eurymeric corrosion-resistant composition of embodiment can contain the imidazole compounds such as pyridine based compound, 2-mercaptobenzimidazole such as 2-pyridine ethanol as substrate driving fit agent.
The preparation of＜eurymeric corrosion-resistant composition 〉
The eurymeric corrosion-resistant composition of present embodiment can mix, stir and prepare by utilizing usual way.In addition, as required, can also use screen cloth, membrane filter etc. to filter.
Eurymeric corrosion-resistant composition discussed above contains novolac resin (A) and emulsion (B).And emulsion (B) contains the phenols (B1) with three (hydroxyphenyl) methane skeleton and the ester compounds that contains the sulfonyl compound (B2) of quinone diazido.In addition, with regard to the eurymeric corrosion-resistant composition, the optical transmission rate of the wavelength 365nm of the etchant resist of thickness 3 μ m is more than 10%.Be more than 10% by making the optical transmission rate, thereby can improve the deciduous of etchant resist.Thereby, utilize the eurymeric corrosion-resistant composition of present embodiment, can realize the raising of deciduous of etchant resist at the recess place of supporting mass.
Formation method and the pattern forming method of＜resist pattern 〉
With reference to Fig. 1 (A)～Fig. 1 (D), Fig. 2 (A)～Fig. 2 (D) and Fig. 3 (A)～Fig. 3 (C), the formation method of the resist pattern of present embodiment, the example of manufacture method having used the pattern forming method of this resist pattern and had a solar cell of the figure that forms by this pattern forming method are described.Fig. 1 (A)～Fig. 1 (D), Fig. 2 (A)～Fig. 2 (D) and Fig. 3 (A)～Fig. 3 (C) is the process profile for the manufacturing process of explanation solar cell.
At first, shown in Fig. 1 (A), such as on the semiconductor substrate 1 (solar cell substrate) of the N-types such as silicon substrate, optionally being coated with mask material composition M.Mask material composition M such as print processes such as can using silk screen print method, ink jet printing method, roller coat print process, toppan printing, woodburytype, hectographic printing method optionally is coated on the surface of semiconductor substrate 1 and becomes diagram shape.After forming mask graph, burn till and make mask material composition M dry.
Then, shown in Fig. 1 (B), with the figure that is formed at the mask material composition M on the semiconductor substrate 1 accordingly, on semiconductor substrate 1 optionally coating contain the P type the Impurity Diffusion composition diffusing agent composition 2 and contain the diffusing agent composition 3 of the Impurity Diffusion composition of N-type.Diffusing agent composition 2 and diffusing agent composition 3 are the compositions that utilize known method to prepare.
Then, shown in Fig. 1 (C), load in such as diffusion furnaces such as electric furnaces and burn till making diffusing agent composition 2 and diffusing agent composition 3 form semiconductor substrate 1 behind the figure, the Impurity Diffusion composition that makes the Impurity Diffusion composition of the P type in the diffusing agent composition 2 and the N-type in the diffusing agent composition 3 is from the surface of semiconductor substrate 1 to semiconductor substrate 1 interior diffusion.It should be noted that, can replace diffusion furnace, and utilize the irradiation of habitual laser to heat semiconductor substrate 1.Like this, the Impurity Diffusion composition of P type will be to semiconductor substrate 1 interior diffusion, and forms p type impurity diffusion layer 4, and in addition, the Impurity Diffusion composition of N-type is to semiconductor substrate 1 interior diffusion, and forms N-type impurity diffusion layer 5.
Then, shown in Fig. 1 (D), such as removers such as use hydrofluorite, mask material composition M, diffusing agent composition 2 and diffusing agent composition 3 are removed.
Then, shown in Fig. 2 (A), utilize thermal oxide etc., on the surface of the side that is formed with p type impurity diffusion layer 4 and N-type impurity diffusion layer 5 of semiconductor substrate 1, form passivation layer 6.In addition, on semiconductor substrate 1 and the face opposite side of a side that is formed with passivation layer 6, utilize known method to form the texture structure with fine concaveconvex structure, form again the silicon nitride film 7 with the effect that prevents sun reflection of light thereon.
Then, shown in Fig. 2 (B), on the passivation layer 6 as supporting mass, the eurymeric corrosion-resistant composition of coating present embodiment, formation for example has the etchant resist 20 of the thickness of 1～30 μ m.The eurymeric corrosion-resistant composition for example can use spin-coating method to coat the surface of passivation layer 6.After the coating of eurymeric corrosion-resistant composition, carry out drying as required and obtain etchant resist 20.
Then, shown in Fig. 2 (C), for example use in the low pressure mercury lamp as light source, high-pressure sodium lamp and the ultrahigh pressure mercury lamp send near the light wavelength 365nm (I line), 405nm (H line), the 436nm (G line) any, across required mask graph M2, optionally etchant resist 20 irradiation dynamic rays L are exposed.It should be noted that, as used dynamic rays L in the exposure, except by above-mentioned low pressure mercury lamp, high-pressure sodium lamp, ultrahigh pressure mercury lamp and the I line, H line and the G line that send, can also use ArF excimer laser, KrF excimer laser, F2 excimer laser, extreme ultraviolet line (EUV), vacuum ultraviolet (VUV), electron beam (EB), X ray and grenz ray isoradial.
Then, shown in Fig. 2 (D), after mask graph M2 is removed, use alkaline-based developer, the tetramethylammonium hydroxide aqueous solution of 0.1～10 quality % for example, under 20～30 ℃ the temperature etchant resist 20 after the exposure being carried out development treatment, the exposed portion of etchant resist 20 is removed., use pure water carry out the water flushing of etchant resist 20, make it dry thereafter.As required, can toast to the etchant resist 20 after the development treatment processing (rear baking).Like this, just can obtain resist pattern 21 faithful to mask graph M2, that have peristome 21a.
Then, shown in Fig. 3 (A), resist pattern 21 is used as mask, the passivation layer 6 to the peristome 21a that is exposed to resist pattern 21 uses the etching solutions such as nitration mixture of hydrofluorite and nitric acid optionally to carry out Wet-type etching.Perhaps, also can implement as required dry-etching processes.Like this, can form the passivation layer 6 that has with resist pattern 21 graphs of a correspondence at semiconductor substrate 1.The part that etching removes of passing through of passivation layer 6 becomes contact hole 6a.In contact hole 6a, expose the regulation zone of p type impurity diffusion layer 4 and N-type impurity diffusion layer 5.
Then, shown in Fig. 3 (B), after the etch processes of passivation layer 6, resist pattern 21 is removed.As the method for removing, can adopt the ashing of having used oxygen plasma to process or used the method for removing of the wet type of stripper.Can implement used the flushing of pure water or lower alcohol etc. process and dry process thereafter.
Then, shown in Fig. 3 (C), among the contact hole 6a on being located at p type impurity diffusion layer 4, for example utilize electrochemical plating and electroless coating method to fill required metal, thereby form the electrode 8 that is electrically connected with p type impurity diffusion layer 4.In addition, similarly among the contact hole 6a on being located at N-type impurity diffusion layer 5, form the electrode 9 that is electrically connected with N-type impurity diffusion layer 5.By above operation, can produce the solar cell 10 of the figure with regulation of present embodiment.
Therefore the eurymeric corrosion-resistant composition of present embodiment can precision form required figure owing to having excellent deciduous and film attenuate inhibition concurrently goodly on the supporting mass that comprises the used for solar batteries substrate.Consequently, can obtain more high performance solar cell.
It should be noted that, in the manufacturing process of above-mentioned solar cell 10, although resist pattern 21 is used for the figure of passivation layer 6 is formed, yet also resist pattern 21 can be used for the figure formation of diffusion layer or electrode, substrate etc.In addition, in above-mentioned solar cell 10, although side has formed texture structure below semiconductor substrate 1, yet also side, the surface of semiconductor substrate 1 that namely is formed with a side of passivation layer 6 form texture structure or without the concaveconvex structure of texture structure in the above.In this situation, in passivation layer 6, form caused concavo-convex by this structure.Eurymeric corrosion-resistant composition according to present embodiment, even the distance cause beginning to etchant resist from the interface of etchant resist and lower floor because this is concavo-convex till, namely, in the thickness of the etchant resist situation about creating a difference, also can reduce the difference of the dissolution velocity of etchant resist for developer solution.Thus, because can obtain the good resist pattern of resolution, therefore also can carry out high-precision graph transfer printing for the irregular passivation layer 6 of this kind tool.
[embodiment]
Below, embodiments of the invention are described, yet these embodiment only are used for illustrating well illustration of the present invention, to the present invention without any restriction.
(preparation of eurymeric corrosion-resistant composition-1)
Novolac resin (A), emulsion (B), sensitizer (D) are dissolved in the solvent (C), prepare embodiment 1,2 and comparative example 1,2 eurymeric corrosion-resistant composition.With embodiment 1,2 and comparative example 1,2 eurymeric corrosion-resistant composition in the content of each composition be shown in Table 1.The content of each composition is the ratio (quality %) for the gross mass of eurymeric corrosion-resistant composition.
The novolac resin of each embodiment and each comparative example (A-1) is and is 5200 compound (A1), is that 7000 compound (A2) mixes the resin that gets equally with having the structure that represented by following formula (5) and Mw having by the structure of following formula (5) expression and Mw.
[in the following formula (5), m: p=36: 64.]
Emulsion (B-a) be by the phenols (B1) of following formula (6) expression, with by 1 of following formula (3) expression, the ester compounds of 2-naphthoquinones-2-diazido-5-sulfonyl compound.It should be noted that, in the ester compounds as emulsion (B-a), with respect to for 1 mole of the phenols (B1) of following formula (6) expression 1, the average mol of 2-naphthoquinones-2-diazido-5-sulfonyl is 2 moles.
Emulsion (B-b) be by the phenols (B1) of following formula (7) expression, with by 1 of following formula (4) expression, the ester compounds of 2-naphthoquinones-2-diazido-4-sulfonyl compound.It should be noted that, in the ester compounds as emulsion (B-b), with respect to for 1 mole of the phenols (B1) of following formula (7) expression 1, the average mol of 2-naphthoquinones-2-diazido-4-sulfonyl is 2.2 moles.
Emulsion (B-c) be by the 2,3,4,4'-Tetrahydroxybenzophenone of following formula (8) expression, with will be by 1 of following formula (3) expression, the R in 2-naphthoquinones-2-diazido-5-sulfonyl compound be substituted by Cl and the ester compounds of compound.It should be noted that, in the ester compounds as emulsion (B-c), for 1 mole of 2,3,4,4'-Tetrahydroxybenzophenone 1, the average mol of 2-naphthoquinones-2-diazido-5-sulfonyl is 2.5 moles.
Emulsion (B-d) is by 2 of following formula (9) expression; 3; the 4-trihydroxybenzophenone, with will be by the sulfonyl compound that contains the quinone diazido (B2) 1 of following formula (3) expression, the R in 2-naphthoquinones-2-diazido-5-sulfonyl compound be substituted by Cl and the ester compounds of compound.It should be noted that, in the ester compounds as emulsion (B-d), do not control with respect to 1 of 1 mole of 2,3,4-trihydroxybenzophenone the molal quantity of 2-naphthoquinones-2-diazido-5-sulfonyl.
The sensitizer of each embodiment and each comparative example (D) is the phenol body (PAMF) of 4-tomatotone.In addition, the solvent of each embodiment and each comparative example (C-1) is propylene glycol monomethyl ether (PM).
[table 1]
(transmissivity measures-1)
Use spinner that the eurymeric corrosion-resistant composition of each embodiment and each comparative example is coated on the silicon substrate.The silicon substrate that is coated with corrosion-resistant composition is loaded on heating plate and 120 ℃ of lower bakings 90 seconds, form the etchant resist of thickness 3 μ m.Then, use light splitting ellipsometer (model VUV-VASE (J.A.Woollam Japan Co., Ltd. system)), each etchant resist is distinguished optionally illumination wavelength 365nm (I line), 405nm (H line), near the light of 436nm (G line), determine the transmissivity (%) of each light.With the results are shown in the table 2 of gained.
(dissolution velocity assessment of indices-1)
For the eurymeric corrosion-resistant composition of each embodiment and each comparative example, form the etchant resist of 3 μ m and the etchant resist of 8 μ m same as the above-mentioned methodly.Then, utilize I line exposing machine (Nikon NSR-2205i14E), in the scope of 0～2000msec, set a plurality of different exposures, to the light of each etchant resist illumination wavelength 365nm (I line).Use dissolution velocity analytical equipment (model RDA-808RB (Litho Tech Japan Co., Ltd. system)) to determine the dissolution velocity (nm/sec) of the etchant resist under each exposure.And, with the maximal value of the dissolution velocity of the etchant resist of the thickness 8 μ m maximal value divided by the dissolution velocity of the etchant resist of thickness 3 μ m, thereby calculate the dissolution velocity index of each etchant resist.According to this result, estimated the deciduous of each embodiment and each comparative example.Evaluation is that situation more than 0.70 is made as well (A) with the dissolution velocity index, and the dissolution velocity index is made as bad (B) less than 0.70 situation.With the results are shown in the table 2 of gained.
[table 2]
As shown in table 2; with regard to the ester compounds of the phenols (B1) that will have three (hydroxyphenyl) methane skeleton and the sulfonyl compound (B2) that contains the quinone diazido as with regard to the embodiment 1 of emulsion (B), 2 the eurymeric corrosion-resistant composition; the dissolution velocity index is compared more near 1 with comparative example 1,2; thereby the difference of the dissolution velocity that is caused by the difference of thickness is little, confirms that thus the deciduous of etchant resist is good.
(preparation of eurymeric corrosion-resistant composition-2)
Novolac resin (A), emulsion (B) and sensitizer (D) are dissolved in the solvent (C), prepare the eurymeric corrosion-resistant composition of embodiment 3～7 and comparative example 3 with the use level of record in the table 3.The content of each composition is the ratio (quality %) for the gross mass of eurymeric corrosion-resistant composition.
[table 3]
In the table 3, (A-2)～(A-6) refer to following resin.
(A-2): have structure (wherein, the m: p=60: 40 by following formula (5) expression.) and Mw be 3000 compound (A3)
(A-3): with above-claimed cpd (A3), with structure (wherein, the m: p=36: 64 that has by following formula (5) expression.) and Mw be that 2150 compound (A4) mixes the resin that gets with 40: 60 (mass ratio)
(A-4): above-claimed cpd (A3) mixed with 50: 50 (mass ratio) with (A4) and resin
(A-5): above-claimed cpd (A3) mixed with 60: 40 (mass ratio) with (A4) and resin
(A-6): above-claimed cpd (A3) mixed with 80: 20 (mass ratio) with (A4) and resin
In the table 3, emulsion (B-e) be by the phenols (B1) of following formula (7) expression, with by 1 of following formula (4) expression, the ester compounds of 2-naphthoquinones-2-diazido-4-sulfonyl compound.It should be noted that, in the ester compounds as emulsion (B-e), with respect to for 1 mole of the phenols (B1) of following formula (7) expression 1, the average mol of 2-naphthoquinones-2-diazido-4-sulfonyl is 2.3 moles.
In the table 3, solvent (C-2) is the diethylene glycol monoethyl ether acetic acid esters.Other composition is identical with table 1.
(transmissivity measures-2)
For the eurymeric corrosion-resistant composition of each embodiment and each comparative example, determine the transmissivity of wavelength 365nm (I line) same as the above-mentioned methodly.With the results are shown in the table 4 of gained.
(dissolution velocity assessment of indices-2)
Eurymeric corrosion-resistant composition for each embodiment and each comparative example determines the dissolution velocity index same as the above-mentioned methodly.With the results are shown in the table 4 of gained.
(thickness dependence)
The eurymeric corrosion-resistant composition of each embodiment and each comparative example is coated on the Si substrate, and the baking of carrying out under 120 ℃ 90 seconds is processed, and forms respectively the etchant resist of 3 μ m, 4 μ m, 4.5 μ m.Then, utilize I line exposing machine (Nikon NSR-2205i14E), in the scope of 0～2000msec, change exposure interimly and expose, the development treatment of using the 2.38%TMAH aqueous solution to carry out 90 seconds.Exposure when measuring exposure section and dissolve fully for each thickness, the thickness dependence of observation exposure (sensitivity).With the variable quantity of the exposure of each thickness be ± 5mJ/cm
2The situation of scope be made as A, will be above ± 30mJ/cm
2The situation of scope be made as B.
[table 4]
As shown in table 4; with regard to the ester compounds of the phenols (B1) that will have three (hydroxyphenyl) methane skeleton and the sulfonyl compound (B2) that contains the quinone diazido as with regard to the eurymeric corrosion-resistant composition of the embodiment 3～7 of emulsion (B); the dissolution velocity index is compared more near 1 with comparative example 3; the difference of the dissolution velocity that is therefore caused by the difference of thickness is little, confirms that thus the deciduous of etchant resist is good.Can confirm that in addition the thickness dependence is also little, even thereby on the irregular substrate of surperficial tool, also can give play to good photoetch characteristic.
For example, for the embodiment that adopts following combination, they also should be contained in the scope of the present invention.
(project 1)
A kind of formation method of resist pattern is characterized in that, comprising:
The eurymeric corrosion-resistant composition is coated on the supporting mass that comprises solar cell substrate and forms the operation of etchant resist, wherein, described eurymeric corrosion-resistant composition contains novolac resin (A) and emulsion (B) and the optical transmission rate of the wavelength 365nm of the etchant resist of the thickness 3 μ m that formed by described eurymeric corrosion-resistant composition is more than 10%, and described emulsion (B) contains the phenols (B1) with three (hydroxyphenyl) methane skeleton and the ester compounds that contains the sulfonyl compound (B2) of quinone diazido;
Above-mentioned etchant resist is optionally shone light and the operation of exposing; And
Above-mentioned etchant resist after will exposing with alkaline solution develops, the operation that exposed portion is removed.
(project 2)
According to the formation method of the resist pattern described in the project 1, wherein, above-mentioned phenols (B1) is by following formula (1) or following formula (2) expression.
[in formula (1), (2), R
B1～R
B5Be the alkyl of hydrogen atom, carbon number 1～10 or the alkyl of ring-type independently of one another; R
B6Be hydrogen atom or methyl; P is 1 or 2.]
(project 3)
According to the formation method of the resist pattern described in project 1 or 2, wherein, the above-mentioned sulfonyl compound (B2) of quinone diazido that contains is by following formula (3) or following formula (4) expression.
[in formula (3) and the formula (4), R is hydrogen atom, chlorine atom or methyl.]
(project 4)
A kind of pattern forming method, it comprises that the resist pattern that the formation method by each described resist pattern in the project 1～3 is formed as mask, carries out etched operation to the supporting mass that comprises solar cell substrate partly.
(project 5)
A kind of solar cell, it comprises the figure that utilizes project 4 described pattern forming methods and form.
(project 6)
A kind of eurymeric corrosion-resistant composition is characterized in that, is used for the manufacturing of solar cell,
Contain novolac resin (A) and emulsion (B), the optical transmission rate of the wavelength 365nm of the etchant resist of the thickness 3 μ m that formed by described eurymeric corrosion-resistant composition is more than 10%,
Wherein, described emulsion (B) contains the phenols (B1) with three hydroxyphenyl methane skeletons and the ester compounds that contains the sulfonyl compound (B2) of quinone diazido.
Claims (6)
1. the formation method of a resist pattern is characterized in that, comprising:
The eurymeric corrosion-resistant composition coated on the supporting mass that comprises solar cell substrate and form the operation of etchant resist, wherein, described eurymeric corrosion-resistant composition contains novolac resin A and emulsion B and the optical transmission rate of the wavelength 365nm of the etchant resist of the thickness 3 μ m that formed by described eurymeric corrosion-resistant composition is more than 10%, and described emulsion B contains the phenol B1 with three (hydroxyphenyl) methane skeleton and the ester compounds that contains the sulfonyl compound B2 of quinone diazido;
Described etchant resist is optionally shone light and the operation of exposing; And
Described etchant resist after will exposing with alkaline solution develops and operation that exposed portion is removed.
2. the formation method of resist pattern according to claim 1, wherein,
Described phenols B1 is by the expression of following formula (1) or following formula (2),
In formula (1), (2), R
B1～R
B5Be the alkyl of hydrogen atom, carbon number 1～10 or the alkyl of ring-type independently of one another; R
B6Be hydrogen atom or methyl; P is 1 or 2.
3. the formation method of resist pattern according to claim 1, wherein,
The described sulfonyl compound B2 that contains the quinone diazido is by following formula (3) or following formula (4) expression,
In formula (3) and the formula (4), R is hydrogen atom, chlorine atom or methyl.
4. a pattern forming method is characterized in that,
Comprise that the resist pattern that will form by the formation method of resist pattern claimed in claim 1 as mask, carries out etched operation to the supporting mass that comprises solar cell substrate partly.
5. a solar cell is characterized in that,
Comprise the figure that forms by pattern forming method claimed in claim 4.
6. an eurymeric corrosion-resistant composition is characterized in that, is used for the manufacturing of solar cell,
Contain novolac resin A and emulsion B, the optical transmission rate of the wavelength 365nm of the etchant resist of the thickness 3 μ m that formed by described eurymeric corrosion-resistant composition is more than 10%,
Wherein, described emulsion B contains the phenols B1 with three hydroxyphenyl methane skeletons and the ester compounds that contains the sulfonyl compound B2 of quinone diazido.
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